反応 #54322

ord-3e50ab561b124247a9b9c228a91b812e

反応方程式

C/C=C/C(=O)Cl
crotonyl chloride
[Na]
sodium
Oc1ccc(Nc2ccccc2)cc1
4-anilinophenol
Oc1ccc(Nc2ccccc2)cc1
4-anilinophenol
O
water
C/C=C/C(=O)Oc1ccc(Nc2ccccc2)cc1
4-Anilinophenyl crotonate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was prepared
  2. 2
    workup.ADDITIONThe addition
  3. 3
    その他The organic layer was separated
  4. 4
    洗浄washed three times with 10 percent sodium hydroxide solution
  5. 5
    乾燥once with water, dried over anhydrous sodium sulfate
  6. 6
    その他to evaporate
  7. 7
    その他The residue was recrystallized from hexane yielding 13.3 grams of product which melted at 73°-76° C.

実験手順

4-Anilinophenyl crotonate was prepared by adding a solution of 11.5 grams of crotonyl chloride in 50 milliliters of benzene to a solution of the sodium salt of 4-anilinophenol which was prepared by dissolving 18.5 grams of 4-anilinophenol in a solution of 4 grams of sodium hydroxide in 100 milliliters of ethanol. The addition was accomplished in 30 minutes and the reaction mixture was stirred for one hour. The mixture was then poured into 150 milliliters of water. The organic layer was separated, washed three times with 10 percent sodium hydroxide solution and once with water, dried over anhydrous sodium sulfate, then allowed to evaporate. The residue was recrystallized from hexane yielding 13.3 grams of product which melted at 73°-76° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04147880uspto-grants-1979_04